摘要
目的建立高效液相色谱法测定乳制品中5-羟甲基糠醛、糠醛、呋喃酮、2-乙酰基呋喃和5-甲基-2-糠醛含量的方法。方法样品经偏磷酸沉淀提取后,过滤滤液在高效液相色谱仪上经C_(18)色谱柱分离,以5%甲醇水为流动相,等度洗脱,紫外检测器检测,采用生乳基质匹配标准曲线,外标法定量糠醛类物质的含量,并监测乳制品中5-羟甲基糠醛含量的变化。结果5种糠醛类化合物在0.01~0.50μg/mL范围内呈线性关系,相关系数(r2)≥0.9980;称样量为10g时,5-羟甲基糠醛和糠醛定量限为3μg/100g,检出限为1.5μg/100g,呋喃酮、2-乙酰基呋喃、5-甲基-2-糠醛的定量限为5μg/100 g,检出限为3μg/100 g,三水平加标样品回收率为:85%~104%,相对标准偏差为1.3%~7.1%(n=7)。乳品在贮藏期间,5-羟甲基糠醛存在下降趋势并趋于平衡,不同包装、不同牛奶中5-羟甲基糠醛含量不同。结论该方法通过基质外标法定量,从特异性、检出限、定量限、方法线性、正确度、重复性6个参数进行验证,其专属性强、准确度高,适用于乳制品中糠醛类物质含量的测定。
Objective To establish a method for the determination of 5-hydroxymethylfurfural,furfural,furanone,2-acetylfuran and 5-methyl-2-furfural in dairy products by high performance liquid chromatography.Methods After extraction and precipitation with metaphosphoric acid,the filtered solution was separated on a C18 column using high performance liquid chromatography with an isocratic elution of 5%methanol-water as the mobile phase.Dectection was carried out using an ultraviolet detector.Furfural compounds were quantified by the external standard method with raw milk to construct the matrix-matched standard curve.Additionally,the changes of 5-hydroxymethylfurfural content in dairy products during storage was investigated.Results The results showed that 5 kinds of furfural compounds exhibited good linearity in the range of 0.01-0.50μg/mL,with correlation coefficients(r2≥0.998).With a sample of 10 g,the limits of quantitation for 5-hydroxymethylfurfural and furfural were 3μg/100 g,and the limits of detection were 1.5μg/100 g.For furanone,2-acetylfuran and 5-methyl-2-furfural,the limits of quantitation and limits of detection were 5μg/100 g and 3μg/100 g,respectively.The recoveries for the three-level spiked samples were 85%-104%.The relative standard deviations were ranging from 1.3% to 7.1%(n=7).During storage,5-hydroxymethylfurfural content in sterilized milk showed a declining trend before stabilizing,the concentration of 5-hydroxymethylfurfural varies depending on the type of packaging and the specific dairy product.Conclusion This method is quantified by matrix external standard method,validated by 6 parameters including specificity,limit of detection,limit of quantitation,method linearity,accuracy and repeatability.It has strong specificity and high accuracy,and is suitable for the determination of furfural content in dairy products.
作者
李秋琴
董立雅
喻东威
黄文强
王颖慧
朱鑫鑫
逯刚
LI Qiu-Qin;DONG Li-Ya;YU Dong-Wei;HUANG Wen-Qiang;WANG Ying-Hui;ZHU Xin-Xin;LU Gang(Inner Mongolia Mengniu Dairy(Group)Co.,Ltd.,Hohhot 011500,China;Key Laboratory of Dairy Quality Digital Intelligence Monitoring Technology,State Administration for Market Regulation,Hohhot 011500,China;Inner Mongolia Arla Foods Dairy Products Co.,Ltd.,Hohhot 011500,China)
出处
《食品安全质量检测学报》
2025年第22期135-142,共8页
Journal of Food Safety and Quality
基金
国家重点研发计划项目(2022YFD1301005)。
关键词
乳制品
高效液相色谱法
糠醛类物质
5-羟甲基糠醛
方法学验证
贮藏
dairy products
high performance liquid chromatography
furfural compounds
5-hydroxymethylfurfural
method validation
storage
